HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Chloride → 1-Hexyl-4-methyl-3-nitro-5-phenyl-2-pyridone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Chloride | HCID 433294 | — |
| Edukt | Tributylphenyltin | HCID 607632 | — |
| Edukt | 1-Hexyl-5-iodo-4-methyl-3-nitro-2-pyridone | HCID 21706525 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 1-Hexyl-4-methyl-3-nitro-5-phenyl-2-pyridone | HCID 21706540 | 72,2% |
Reaktionsschritte
A mixture of bis(triphenylphosphine)Pd(II) chloride (0.014 g), lithium chloride (0.067 g), 1-hexyl-5-iodo-4-methyl-3-nitro-2-pyridone (0.15 g, 0.41 mmol) and phenyltributyltin (0.11 mL, 0.62 mmol) in THF (15 mL) was heated under reflux for 2 days. The mixture was cooled, diluted with ethyl acetate, and washed with aqueous potassium fluoride and water. The organic phase was dried, filtered and evaporated. Chromatography of the residue over silica gel (petroleum ether/methylene chloride 1/1 to methylene chloride is gradient) gave 1-hexyl-4-methyl-3-nitro-5-phenyl-2-pyridone (0.093 g, 72%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06268365B1 |
| Quelldatensatz | uspto-grants-2001_07 |
| ORD ID | ord-9b7e98136a404e32892c393e44a41e3b |
| Quellennotiz | uspto-grants-2001_07 |